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Synthetic Fibers and Thermoplastic

Short-Fiber-Reinforced Polymers: Properties

and Characterization

Christoph Unterweger,1 Oliver Bru

€ ggemann,2 Christian Fu
€ rst1
Kompetenzzentrum Holz GmbH (Wood K plus), Division of Wood Polymer Composites, Linz, Austria

Johannes Kepler Universita€t Linz, Institut fu€r Chemie der Polymere (ICP), Leonding, Austria

Among the synthetic fibers, glass fibers (GF) are most All the data are taken from scientific literature or mate-
widely used in thermoplastic short-fiber-reinforced rial data sheets provided by the suppliers. For better com-
polymers (SFRP), as they offer good strength and stiff-
ness, impact resistance, chemical resistance, and ther-
parability only data of injection molded specimens (or
mal stability at a low price. Carbon fibers (CF) are compression molded specimens, when no literature on
applied instead of GF, when highest stiffness is injection molded specimens is available) are included.
required. Other types of synthetic fibers like aramid Due to the lack of data concerning the fiber-reinforcement
(AF), basalt (BF), polyacrylonitrile (PAN-F), polyethylene of other thermoplastic materials, a comparison of various
terephthalate (PET-F), or polypropylene fibers (PP-F)
are rarely used in SFRP, although they offer some
fiber types could be done only for SFRPP. For comparison
advantages compared with GF. The aim of this article of material property data, the Ashby plot [1] was chosen
is, to give an overview of various fiber types with as means of presentation. Plots as tensile strength versus
regard to their mechanical properties, densities, and tensile modulus for reinforcing fibers, matrix polymers,
prices as well as the performance of their thermoplas- and fiber-reinforced composites are included in this over-
tic composites. The mechanical properties are pre-
sented as Ashby plots of tensile strength versus
view. Because of the growing interest in fiber-reinforced
tensile modulus, both in absolute and specific (abso- materials for lightweight structural design, Ashby plots for
lute value divided by density) values. This overview specific property values are illustrated, too.
also focuses on modification of fiber/matrix interac-
tion, as interfacial adhesion has a huge impact on
composite performance. A summary of established FIBERS
methods for characterization of fibers, polymers, and
composites completes this article. POLYM. COMPOS., This overview focuses on synthetic fibers used for
35:227–236, 2014. V C 2013 Society of Plastics Engineers reinforcing thermoplastic matrices. For comparison, prop-
erties of CeF are included, too. Throughout this article,
the term “synthetic fibers” refers to AF, BF, CF, and GF.
INTRODUCTION Other man-made fibers based on noncellulosic materials
like PAN, PET, and PP are rarely used in SFRP and only
Short-fiber-reinforced polymers (SFRP) (see Table 1 included for comparison. When mentioned, these fibers
for abbreviations) have become more and more popular are referred to as PAN-F, PET-F, and PP-F, respectively.
in various application fields like automotive or building The term “CeF” includes plant-based fibers (e.g. jute,
and construction industry, as they combine the advantages hemp, kenaf, sisal, flax, and wood) and man-made fibers
of polymers like good impact resistance and low weight based on cellulosic material (e.g. Kraft pulp, unbleached
with the high stiffness and strength of reinforcing fibers. cellulose, regenerate cellulose).
Ease of processing, low price, and worldwide accessibility Synthetic fibers outperform CeF in their mechanical
make thermoplastic SFRP suitable for mass production. properties (see Fig. 1) and show less variation in product
quality. Another advantage of synthetic fibers is their bet-
ter thermal stability, which allows higher processing tem-
peratures, while CeF are known to show a strong
Correspondence to: Christoph Unterweger; decrease of mechanical properties under the influence of
e-mail: c.unterweger@kplus-wood.at
DOI 10.1002/pc.22654
high temperatures [2, 3]. CeF also offer an advantage in
Published online in Wiley Online Library (wileyonlinelibrary.com). terms of processing behavior, as they are known to cause
C 2013 Society of Plastics Engineers
V less equipment wear [2, 4].

TABLE 1. Abbreviations used in the text.

Abbreviation Explanation

AF Aramid fibers
AFM Atomic force microscopy
BF Basalt fibers
CeF Cellulose-based fibers
CF Carbon fibers
DMA Dynamic mechanical analysis
DSC Differential scanning calorimetry
EP Epoxy resin
GF Glass fibers
IFSS Interfacial shear strength
PA Polyamide
PAN-F Polyacrylonitrile fibers
PE-HD Polyethylene high density
PE-LD Polyethylene low density FIG. 1. Ashby plot presenting absolute tensile strength versus tensile
PEEK Polyether ether ketone modulus for various fiber types. [Color figure can be viewed in the
PET Polyethylene terephthalate online issue, which is available at wileyonlinelibrary.com.]
PET-F Polyethylene terephthalate fibers
PP Polypropylene
However, prices of dosable natural fibers and man-made
PP-F Polypropylene fibers
PPS Polyphenylene sulfide cellulose fibers are usually in the range or slightly above
PS Polystyrene the price levels of PP and GF [37]. In contrast to some
PSU Polysulfone reports that BF are cheaper than GF [40–42], actual mar-
PUR Polyurethane ket prices for short GF are much lower than for BF. The
PVC Polyvinyl chloride
most expensive fibers are AF and CF with prices ranging
SEM Scanning electron microscopy
SFFT Single fiber fragmentation test from 20 to 40 e/kg for common types and 80 to 103 e/kg
SFPT Single fiber pull-out test for the most expensive types with special coatings.
SFRP Short-fiber-reinforced polymers To illustrate the mechanical properties of various fiber
SFRPP Short-fiber-reinforced polypropylene types, Ashby plots of tensile strength versus tensile modu-
TEM Transmission electron microscopy
lus were chosen. Ultra-high modulus carbon fibers were
TGA Thermogravimetric analysis
wt% Weight percent not included as no literature for the use of these fibers in
XPS X-ray photoelectron spectroscopy thermoplastic composites was found. All data were taken
XRD X-ray diffraction from the references indicated in Table 3. Due to their var-
iability of mechanical properties, reported minimum and
maximum values were used for natural fibers. For man-
Table 2 provides some general information on the den- made fibers, which are known to meet quite narrow toler-
sities and current prices of the various materials included ances for a specific grade, arithmetic mean values were
in this overview. The significant differences of synthetic used.
fibers in comparison with CeF are apparent from Table 2. Figure 1 shows that CF exhibit the highest tensile
The densities of synthetic fibers are higher with a wide modulus and tensile strength with values ranging from
range from 1.40 to 2.80 g/cm3 versus 1.30 to 1.55 g/cm3
for CeF. Only the little used PAN-F, PET-F, and PP-F
have lower densities than CeF. Furthermore, the prices
for synthetic fibers are higher than that for natural fibers.

TABLE 2. Densities and prices of PP and various synthetic and

cellulose-based fibers.

Material Density (g/cm3) Price (e/kg)

PP 0.90–0.92 [5–10] 1.3 [11]

AF 1.39–1.46 [2, 6, 12–18] 20–80 [19]
BF 2.56–2.80 [20–23] 4.0–6.0 [24]
CF 1.70–1.80 [2, 7, 8, 14, 15, 25–28] 23–36 [29]
GF 2.50–2.70 [7, 8, 14–16, 22, 25, 30] 1.0–1.5 [31]
PAN-F 1.18 [32] 5.0–7.0 [33]
PET-F 1.38 [13, 34]
PP-F 0.91 [35] 3.0–6.0 [36] FIG. 2. Ashby plot presenting specific tensile strength versus specific
CeF 1.30–1.55 [15, 16, 37–39] 0.3–1.5 [37] tensile modulus for various fiber types. [Color figure can be viewed in
the online issue, which is available at wileyonlinelibrary.com.]

228 POLYMER COMPOSITES—2014 DOI 10.1002/pc

TABLE 3. References for the tensile property data of fibers presented in Figs. 1 and 2.


[2, 13, 14, 16–18] [2, 7, 8, 14, 16, 22, 25, 30] [2, 7, 8, 14, 16, 25–28] [2, 7, 8, 14, 16, 22, 25, 30, 43] [32] [34] [35] [2, 37, 38, 44–46]

210 to 240 GPa and 2,000 to 4,900 MPa, respectively. mers presented here, with PP and PE-HD showing similar
Next in line in terms of stiffness are AF with tensile mod- properties and both outperforming PE-LD. All other poly-
ulus values ranging from 62 to 160 GPa. The quite nar- mers show comparable performance with strength and
row margin of tensile strength values from 2,920 to 3,600 modulus values for all polymers varying over wide
MPa is approximately in the middle of the wider ranging ranges. In terms of specific properties the polyolefins
values for GF and CF. In terms of absolute tensile modu- almost close the gap to the other polymers due to their
lus values GF are at the lower end of the corresponding lower densities. As can be seen in Fig. 4, PP even reaches
values for AF. BF show tensile modulus values similar to the lower bound values of PVC and PET. These good
GF, but are slightly outperformed in terms of tensile specific properties in combination with its low price and
strength. Compared with synthetic fibers, CeF exhibit ease of processing constitute PPs predominance among
lower tensile modulus and tensile strength values, with the matrix polymers. The prices for primary thermoplastic
only kenaf and hemp reaching modulus values similar to matrix materials are illustrated in Table 5. Much lower
those of BF and GF. Tensile properties of PAN-F are at prices can be found for recycled polymers [11].
the lower end of the range of CeF. The lowest modulus
values are found for PET-F and PP-F. As fiber densities
range from 0.90 to 2.80 g/cm3, there are differences
between the absolute values illustrated in Fig. 1 and the The properties of the composites mostly depend on the
specific values in Fig. 2. fiber and matrix properties, along with interfacial adhe-
sion. A good interfacial adhesion guarantees an effective
POLYMER MATRICES transfer of stress from the matrix to the reinforcing fiber
The mechanical properties of composite materials not One concept for describing interfacial adhesion is the
only depend on the reinforcing fibers, but also on the calculation of the critical fiber length. If the fiber length
matrix polymer. Therefore, tensile properties of com- is shorter than the critical value, the fiber is pulled out
monly used thermoplastic polymers like PP, PE-HD, PE- from the matrix due to tension force, and the composite
LD, PA6, PA6.6, PET, PVC, and PS as well as EP, the tensile strength is mainly determined by the interfacial
most widely used thermoset, are presented. As density adhesion. If the fiber length is longer than the critical
values range from 0.90 to 1.40 g/cm3 (Table 5) absolute value, the fiber is broken and the strength of the compos-
(Fig. 3) and specific tensile properties (Fig. 4) are illus- ite is determined by the fiber tensile strength [30].
trated in Ashby plots. All data were taken from the refer- As fiber length is dramatically reduced during process-
ences indicated in Table 4. ing of SFRP, the critical fiber length must be decreased
Figure 3 shows that with regard to absolute properties by promoting the interfacial adhesion [61]. To ensure
polyolefin matrix polymers are inferior to all other poly- appropriate interfacial interaction, fibers are usually

FIG. 3. Ashby plot presenting absolute tensile strength versus tensile FIG. 4. Ashby plot presenting specific tensile strength versus specific
modulus for various matrix polymers. [Color figure can be viewed in tensile modulus for various matrix polymers. [Color figure can be viewed
the online issue, which is available at wileyonlinelibrary.com.] in the online issue, which is available at wileyonlinelibrary.com.]

DOI 10.1002/pc POLYMER COMPOSITES—2014 229

coated with a sizing containing a coupling agent. Fiber TABLE 5. Densities and current market prices of thermoplastic
sizings are available for certain kinds of polymers. CF are polymers.
available with sizings for composites with PA, PUR, EP,
Material Density (g/cm3) Price (e/kg)
or high-temperature polymers like PSU, PPS, and PEEK
[75]. AF are available with PUR and PET sizings [12]. PE-HD 0.94–0.96 [9, 47–51] 1.29–1.35 [11]
As GF are much cheaper and more widely used, there is PE-LD 0.91–0.93 [9, 52, 53] 1.27–1.35 [11]
a larger variety of sizings available, including even siz- PP 0.90–0.92 [5–10] 1.29–1.34 [11]
PET 1.34–1.39 [58, 59] 1.38–1.50 [11]
ings for PP and PE matrices [76]. The coupling agents in
PA6 1.12–1.14 [9, 61, 62] 2.45–2.65 [11]
GF sizings are usually silane-based with functional groups PA6.6 1.13–1.15 [9, 14, 65] 3.10–3.20 [11]
varying, depending on the matrix polymer used [30, 61, PVC 1.36–1.39 [66–68] 1.16–1.30 [11]
76]. The same coupling agents can be used for BF. PS 1.04–1.08 [9, 69–71] 1.46–1.63 [11]
Ref. 61 reports a comparison of silane-based coupling
agents in PA/BF composites.
Often an additional coupling agent is used to further cation. In these so-called self-reinforced polymeric mate-
improve interaction between fiber and matrix. The most rials the same polymer forms both the matrix and the
commonly used coupling agents, especially in polyolefin- reinforcing phases. Because of the identical chemical
based composites, are maleic anhydride grafted deriva- nature of the matrix and the filler, exceptional interfacial
tives of the matrix polymer. These coupling agents are adhesion is obtained in these composites [98–101].
known to work very well in glass-fiber reinforced materi-
als, but are used in combination with other fiber types,
too [6, 9, 41, 44, 77–81]. Ref. 41 describes the production
of coupling agents by grafting maleic anhydride onto PROCESSING
C5C bonds containing hydrocarbon molecules like sun- As extrusion is the preferred compounding technique,
flower oil, linoleic acid, or glycerine monooleate. most research is focused on using twin screw extruders for
Beside the use of coupling agents, the fiber/matrix inter- preparation of SFRP compounds [7, 8, 25, 26, 30, 40, 61,
action can be improved by fiber surface modification. The 102–107]. For research in smaller scale, kneaders (labora-
physical interaction can be improved by increasing the tory internal mixers) are used quite frequently. In order to
roughness of the fiber. Ref. 74 describes a method for sur- reduce fiber breakage during compounding usually the
face treatment of CF with ammonia solution, while Ref. 82 polymer is fed into the equipment first and the fibers are
depicts roughening of AF surface by bromination. added to the melted polymer [27, 28, 41, 79, 108].
More widely used methods aim at the functionalization Specimens for mechanical testing are generally produced
of the fiber surface. For AF and CF acidic oxidation [83– by injection molding [7, 8, 25, 26, 30, 40, 54, 61, 102, 103,
87], fluorination [87, 88], and plasma treatment [27, 89– 106, 109–111], but also literature on hot-pressing and com-
92] are described. For CF also ozone treatment [93] or pression molding techniques can be found [13, 27, 28, 108].
electrochemical oxidation [85, 87] are used. Preparation For self-reinforced polymeric materials these conven-
of CF containing acidic or basic surface functionalities by tional techniques usually cannot be used, because of the
different heating and oxidation programs is described in similar melting temperatures of the matrix polymer and
Refs. 94 and 95. Ref. 82 reports the reaction of AF with the filler. Various methods for processing of these materi-
dimethyl sulfoxide and NaH followed by the coupling of als are described in Refs. 98 and 99.
bromoacetic acid or epichlorohydrin onto the fiber sur- Shearing stress during compounding and injection
face. Surfaces of BF and GF are usually modified by cou- molding causes a reduction of fiber length to a few 100
pling of silanes [61]. mm, almost regardless of the initial length [61]. Due to
Before a certain surface treatment method can be increased fiber-fiber interaction and fiber-equipment wall
applied, the sizing should be removed. This can be contact, fiber length decreases with increasing fiber con-
achieved by annealing [61] or by washing with acetone tent [7, 8, 25, 30, 54, 65, 109–111] and decreasing fiber
[83, 96, 97]. What must be considered is that the sizing diameter [54, 65]. Furthermore, process parameters (e.g.
not only includes a coupling agent but several other com- screw speed, processing temperature, injection speed)
ponents protecting the fibers and assuring processability. influence the fiber length distribution as well as the fiber
In the last couple of years a new family of composite orientation distribution, which have a huge impact on the
materials emerged, which exhibits excellent interfacial mechanical properties of the composite [30, 112–114].
adhesion without any coupling agents or surface modifi- Changes in fiber diameter during processing are not

TABLE 4. References for the tensile property data of the various matrix polymers presented in Figures 3 and 4.


[47–53] [5–8, 10, 54–57] [40, 58–60] [14, 61–65] [66–68] [69–71] [14, 72, 73]

230 POLYMER COMPOSITES—2014 DOI 10.1002/pc

techniques). The absolute properties are shown in Fig. 5,
specific properties are not illustrated, as composite den-
sities vary in a quite narrow range around 1 g/cm3. All
data were taken from the references indicated in Table 6.
In accordance to the fiber properties, PP/CF compo-
sites show by far the highest tensile modulus values.
Nevertheless, in terms of strength PP/CF composites are
surpassed by most GF composites, although the strengths
of these fiber types are very similar. This can be attrib-
uted to more optimized fiber/matrix adhesion and proc-
essing conditions in PP/GF. In contrast to this general
trend, Ref. 25 reports a comparison of PP/CF and PP/GF
processed and tested under identical conditions with CF
composites showing higher strength and modulus. In
FIG. 5. Ashby plot presenting absolute tensile strength versus tensile accordance with fiber properties, tensile strain is higher in
modulus for SFRPP. [Color figure can be viewed in the online issue,
which is available at wileyonlinelibrary.com.]
GF composites.
The most surprising results are the poor properties of
PP/BF composites. While BF show mechanical properties
reported for synthetic fibers, decreasing diameters of nat- comparable to those of GF, their composites with PP are
ural fibers can be observed [114–116]. outperformed by all fiber types, with specific strength
even inferior to neat PP. But, what must be considered is,
COMPOSITES that data for PP/BF composites are based on only two
reported sources, with fiber content being on the lower
limit of 20 wt% and specimens being produced by com-
Tensile Properties
pression molding. Nevertheless, from the reported proper-
The fiber and matrix materials used have a main influ- ties it is obvious, that fiber/matrix interaction in PP/BF
ence on mechanical properties of SFRP. Nevertheless, composites is very poor. Similar results can be found in
other parameters like interfacial adhesion, fiber length, Ref. 40, where GF and BF composites with PET matrix
and processing conditions affect the performance of are compared. With addition of BF the tensile strength is
SFRP. Therefore, superior fiber properties are not always little increased compared with the pure matrix, but there
reflected in composite properties. is a significant improvement in tensile strength with
Strength and modulus of polymers generally increase increasing GF content. A reinforcing effect of BF can be
when fibers are added, while the elongation is drastically observed in flexural strength as well as in tensile and
reduced. With increasing fiber content the composite flexural modulus, although they are still inferior com-
properties further follow these trends, even though a pared with the corresponding PET/GF composites. Rein-
decrease in strength is reported at high fiber contents forcement of PA6 with BF is reported in Ref. 61. Using
[109, 110]. coupling agents developed for PA/GF composites, rein-
As most scientific literature could be found on tensile forcement with BF results in a massive improvement in
properties, an Ashby plot of tensile strength versus tensile strength and modulus.
modulus is chosen for comparison of composite proper- As only data of compression molded specimens are
ties. Studies on correlation between tensile and flexural available for PP/AF and PP/PET-F composites [13], it is
properties are reported in Refs. 54 and 65. To reduce the difficult to make a statement about their mechanical per-
influence of processing parameters, only data obtained formance compared with other SFRPP. Nevertheless, in
from injection molded specimen of composites with fiber comparison with other composites investigated in the same
contents between 20 and 40 wt% are illustrated in the study [13], PP/AF composites show the best mechanical
Ashby plot below. However, since no such data were properties, outperforming PP/GF and PP/Sisal in terms of
available for PP/AF, PP/BF, and PP/PET-F, data of com- tensile strength and modulus as well as maximum strain.
pression molded specimen are used for these materials. PP/PET-F composites show modulus and strength values
No suitable data are available for short PP-F (due to the slightly above PP/Sisal, but inferior to PP/AF and PP/GF. In
similar melting temperatures of the matrix and the fiber, terms of maximum strain PP/PET-F composites clearly out-
all-PP composites cannot be processed using conventional perform PP/AF, PP/GF and PP/Sisal.

TABLE 6. References for the tensile property data of SFRPP presented in Fig. 5.


[5, 6, 10, 54–57] [13] [41, 117] [25, 118, 119] [6, 25, 54, 111, 120–124] [125] [13] [45, 126–132]

DOI 10.1002/pc POLYMER COMPOSITES—2014 231

Performance of CeF composites is in accordance with ded length (L) and the fiber diameter (df) are required for
the respective fiber properties. Slight improvements in the calculation of the IFSS [IFSS 5 F/(df 3 p 3 L)].
strength and modulus can be observed with upper bound Knowing the single fiber tensile strength (rf), the critical
values of PP/CeF overlapping with the lower end of PP/ fiber length [Lc 5 (df 3 rf)/(2 3 IFSS)] can be calcu-
GF composites. Surprisingly good properties can be found lated. The embedded length must be kept low (shorter
for PP/PAN-F with tensile strength being superior to PP/ than Lc) in order to achieve debonding and not fiber
CF and PP/CeF. breakage [7, 25, 40, 55, 74, 77, 103, 106, 134–137]. In
the SFFT a single fiber is embedded in a dumbbell-
shaped specimen, which is subjected to a tensile load.
Impact Properties
The loading process continues until the fiber fragments
Due to the variety of instrumental setups and test con- are so short that the induced stress no longer reaches the
ditions as well as the wide ranging values for impact fiber tensile strength and the fiber fragmentation process
properties of matrix polymers, it is difficult to give a ceases. The critical fiber length is obtained from the lon-
comprehensive overview of the impact behavior of vari- gest fragment length. Refs. 77, 134, and 135 compare
ous fiber types. Ref. 37 compares the unnotched Charpy results of micromechanical tests with the mechanical
impact strength of various CeF-based PP composites, PP/ properties of actual composites. It is important to choose
GF and neat PP. While PP/GF composites outperform all an adequate test configuration, where stress distribution is
but one PP/CeF composites, they do not reach the impact similar to that in the real composite [133].
strength of unnotched PP specimens. Ref. 13 reports The fiber/matrix interaction can also be characterized
notched Izod impact strengths of PP reinforced with vari- by SEM images of fracture surfaces. Proper adhesion can
ous fiber types at 125 and 230 C. GF are superior to be identified by good wetting of the fiber and little or no
CeF, but are clearly surpassed by AF and PET-F at pull-out holes, while separation of fiber and matrix is
125 C. Contrary to AF and PET-F, GF completely retain visible in case of weak interfacial bonding [8, 25, 41, 56,
their impact strength at 230 C. Higher notched Charpy 61, 79, 88]. In Ref. 138 the critical fiber length is calcu-
impact strength is reported for PP/GF compared with PP/ lated from SEM images of fracture surfaces. The 10 max-
CF [7]. The highest impact strengths (Charpy notched imum lengths of pulled out fibers are averaged as half of
and unnotched) of SFRPP could be found for PP/PAN-F the critical fiber length.
composites [125]. Also Raman spectroscopy is used to quantify interfacial
adhesion. The method is based on the shift of the Raman
CHARACTERIZATION peaks to lower frequency when the fiber is subjected to an
applied strain. Raman spectroscopy is mostly used for CF
[72, 139, 140], but also studies on AF are reported [141].
Mechanical Properties
Tensile (EN ISO 527, ASTM D-638 M), flexural (EN
Fiber Length and Diameter
ISO 178, EN ISO 14125, ASTM D-790 M), and impact
testing (EN ISO 179, EN ISO 180, ASTM D-256) accord- Before the fiber length in a composite can be meas-
ing to standard methods are used to analyze mechanical ured, the matrix polymer has to be removed. Two meth-
properties of composites and matrix polymers, although ods can be found in scientific literature. In case of fibers
most data can be found on tensile properties. Fibers are with sufficient thermal stability, the matrix polymer can
generally characterized by their tensile strength and ten- easily be removed by pyrolysis at 400 to 600 C for sev-
sile modulus. eral hours [7, 8, 25, 30, 54, 55, 61, 102, 103, 105, 107,
109–111, 142, 143]. In Ref. 142 an explicit embrittlement
of GF during pyrolysis was detected, which may cause
Fiber/Matrix Interaction
fiber degradation in following handling steps.
A common method is to derive information on interfa- If fibers with insufficient thermal stability (e.g. CeF or
cial adhesion from macroscopic composite properties like AF) or polymers that leave a carbon residue are used, the
tensile strength, impact strength or water absorption. matrix has to be removed by extraction using an appropri-
However, since such composite properties are influenced ate solvent. In Refs. 40 and [106], BF and GF were
by other factors as well (e.g. fiber orientation, process- recovered from PET composites by dissolving the matrix
ing), their validity to evaluate interfacial adhesion is lim- in a mixture of phenol (60 wt%) and 1,1,2,2-tetrachloro-
ited. To overcome this shortage, various micromechanical ethane (40 wt%). PA6.6 can be removed from composites
techniques to measure IFSS directly have been developed. with CF by dissolution in formic acid [144]. Polyolefin
An overview of various micromechanical test methods is matrices are usually removed by extraction in boiling
given in Ref. 133. SFPT and SFFT, the most common xylene [78, 114, 115, 145].
micro-mechanical test methods, are described in detail in Fiber length can be measured by optical microscopy
Ref. 134. In SFPT the force to pull a single fiber out of [7, 8, 25, 30, 40, 54, 55, 61, 85, 102, 103, 105, 106, 109–
the matrix is measured. Beside this force (F), the embed- 111, 115, 143] and SEM or TEM for very small fibers

232 POLYMER COMPOSITES—2014 DOI 10.1002/pc

like vapor-grown CF [104, 107, 146]. To achieve an TABLE 7. Enthalpies of hypothetical 100% crystalline polymers.
adequate fiber length distribution, usually a few hundred
Polymer DHm0 [J/g] Source
fibers are analyzed. Use of automatically measurement
systems is described in Refs. 78, 104, and 114. PP 138, 190, 207, 209 [41, 56, 88, 108, 136, 156, 158, 159]
All the methods mentioned above can also be used for PE 293 [159]
measuring fiber diameters. However, measurements of PET 118, 140–145 [106, 157, 159]
fiber diameter are normally just performed, when the PA6 230 [159]
PA66 255, 300 [159]
exact diameter of a single fiber is needed (e.g. for calcu-
lation of IFSS from micromechanical tests).
The thermal stability of various types of fibers and
Fiber Composition and Surface matrix polymers is usually measured by TGA [28, 56, 88,
111, 145, 155]. Various sources report better thermal sta-
For analysis of fiber surface composition, which is
bility of composites compared with the pure matrix mate-
often performed to investigate the effect of surface treat-
rial [28, 56, 111]. For composites containing thermally
ment methods, XPS is the most widely used method [27,
stable fibers, the actual content of the reinforcing material
74, 83–85, 90–93, 147–149]. Ref. 148 compares XPS and
can be measured by TGA [28, 56, 111, 155].
XRD data of CF. While XPS reflects the surface proper-
A method for analysis of thermomechanical properties
ties, XRD gives information about the bulk structure.
of polymers and fiber-reinforced composites is DMA.
Therefore, XRD hardly reflects effectiveness of surface
Various instrumental setups like single cantilever or dual
treatment, but can be used for characterization of bulk
cantilever, bending, or tensile mode are reported. Most
properties [148, 150]. Differences in crystalline structure
experiments are performed using a temperature sweep
of various CF types can be characterized by Raman spec-
program with heating rates of 2 or 5 C/min. Sinusoidal
troscopy [150, 151]. Functional groups on fiber surfaces
force or strain are usually applied with frequencies of 1
can be identified by infrared spectroscopy. Methods are
or 10 Hz [28, 61, 79, 152, 160–162]. The measured stor-
described for AF [80, 82, 84, 88, 152], BF [61], CF [85,
age modulus (E’) correlates with the modulus from
153, 154], and GF [155].
mechanical testing and can be used to compare stiffness
Analysis of surface topography, which can be used for
of various materials over a wide temperature range.
characterization of the effect of surface treatment methods
Sometimes the glass transition temperature is derived
on surface roughness, is usually performed by AFM [74,
from the onset of the decrease in the storage modulus,
137, 149] or SEM [95, 137, 155].
although this is better characterized by the maximum of
Specific surface area can be measured by BET gas
the loss modulus (E00 ) or the loss factor (tan d). The sensi-
adsorption [85, 86, 150], while concentration of acidic
tivity to glass transitions is said to be one decade higher
and basic groups is measured by NaOH or HCl uptake
for DMA compared with DSC [162]. Using time-
respectively [85, 86]. Zeta potential measurements can be
temperature-superposition, DMA can further be used to
applied for characterization of acidic and basic surface
predict long-term creep behavior [163–166].
functionalities on CF [94, 95].
Various methods for contact angle measurements are
used to determine the surface energy and to quantify
effectiveness of several surface treatment methods [85, The comparison of the tensile properties of various
88, 92, 94, 95, 137]. By measuring the contact angles to fiber types used in SFRP shows a potential for partial
test liquids of known surface energies, the fiber surface substitution of GF. AF and CF clearly outperform GF in
energy including its polar and dispersive components can terms of stiffness and specific tensile strength. BF show
be calculated [74, 88, 94, 95, 137, 149]. tensile properties comparable to those of GF and even
CeF can compete with GF, especially when the difference
in fiber densities is taken into account. However, superior
Thermal Analysis
fiber properties are not always reflected in composite
The most prominent method for thermal analysis is properties. GF reinforcement yields the highest tensile
DSC, which can be used for determination of the degree strength values (even higher than CF) and even the tensile
of crystallinity [41, 88, 106, 108, 136, 156, 157]. To modulus values are superior to all other fiber types except
obtain the required enthalpy, the sample is first melted to for CF. The main reasons are the more optimized fiber/
erase thermal history, then cooled at a defined rate, and matrix interaction and processing conditions for GF-
usually heated again at a defined rate. The data are calcu- reinforced composites. Therefore, the main task must be,
lated from the crystallization peak in the cooling step or to improve the fiber/matrix interaction and processing
from the melting peak in the second heating cycle. Com- conditions for all fiber types. This is especially interest-
mon cooling and heating rates are 10 C/min [41, 88, 106, ing, as all fiber types offer typical characteristics that
108, 156, 157]. The enthalpies of hypothetical 100% crys- might be advantageous for specific applications. CF,
talline polymers are given in Table 7. although they are very expensive, are already widely

DOI 10.1002/pc POLYMER COMPOSITES—2014 233

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